High-pressure contacting apparatus



March 10, 1953 w. KUENTZEL ET AL 2,631,091

HIGH-PRESSURE CONTACTING APPARATUS Filed May 21, 1949 2 SHEETS--SHEET 1 RELAY 66 47; 54 55 TIMER RELAY March 10, 1953 w. E. KUENTZEL ET AL 2,631,091

HIGH-PRESSURE CONTACTING APPARATUS 2 SHEETSSHEET 2 Filed May 21, 1949 INVENTORS.

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Patented Mar. 10, 1953 HIGH-PRESSURE CONTACTING APPARATUS Ward E. Kuentzel, Whiting, End and Edmund Field, Chicago, 111., assignors to StandardOil Company, Chicago, Ill., a corporation of Indiana Application May 21, 1949, Serial No. 94,718

.12 Claims.

This invention .relates to .hi h pressure contacting apparatus and it pertains, more particu- .larly, to improved apparatus for effecting contact between two separatephases, one of which being a liquid and the other being either gaseous, liquid. .or a solid, under extremely high pressure conditions and under closely controlled tempera ture conditions.

j An object of the invention is to provide an apparatus which is particularly suitable for smallscale or laboratory use in obtaining critically l close control in the contacting of two immiscible phases-at pressures in the range of,1,000 to 15,000 pounds per square inch and at "temperatures up to 750? F. orv higher. .A particular object is to provide an'improvedstirring mechanism entirely closed within thereactor space and controllable with a precision which has heretofore been unobtainable in reactors of this type. Another object is to provide a heating and temperature control system from which the contacting apparatus per se is readily separable. A further object is to provide an improved method and means for recycling and/or introducing gases into liquids at extremely high super atmospheric pressure. Other objects will be apparent as the detailed description of the invention proceeds.

. In accordance with our invention, an upright vopen-ended contactor support is provided with heating and temperature control elements so that the contactor itself is not encumbered by the heating element but may simply be inserted into it. The contactor, or reactor, is preferably provided with a thermowell at..its base, and it is usually. of utmost. importance that separate phases immediately adjacent this thermowell be mixed or agitated at a determinable and precisely controllable rate. To accomplish this mixing or contacting, a plunger-type mixer is reciprocally mounted in the contactor so that in its lowermost position it comes in close proximity to the base of the reactor and the thermowell, and in its upper position it. approaches the .top of a liquid phase in the contactor .oremerges from the top of said liquid phase, depending upon Whether or not it is desired to obtain a mixing of an upper gaseous phase with a lower liquid phase or phases. The stirrer is positively actuated, .bothupwards and downwards, bythe electromagnetic effect of two separate solenoids on. a. magnetic core which is fixedly connected .to. the stirrer. .The. upper solenoidfunctions to positively. .raisethe. core and stirrer and the lower coil to positively. lower the coreand stirrer in accordance with an electronic timing mechanism of any type known to the art so that both; the frequency :and the speedotthe upward and downward movements canbe controlled withgreat precision. The positive.'downward stroke of the core and mixer-is perhaps of even greater. effectiveness than the upward movement thereof but itis essential that movement in both directions be positively actuated-endearefully controlled.

The invention prov-idesnot only for positive and closely controlled-stirring or mixing action in both upward and downward directions, but it also provides a means for simultaneously or alterand a gas conduit is provided for conducting gas from the upper part of the chamber to the base thereof. The sharp downward movement of the core causes thevalve toopen andpredetermined 'amountof gasto be trapped above the valve; the sharp or. controlled upward movement of the core forces the'entrapped gas through the conduit to the base of the contactor or reactor.

The inventionv will be more clearly understood from the following detailed description of a specific example thereof, read in conjunction with the accompanying drawings, inwhich Figure 1 is a schematic view of our improved apparatus in vertical section.

. Figures 2, 3 and 4 are detailed. views illustrating gas recycle features.

As an example of the apparatus of our invention we will describe a laboratory reactor designed to obtain closely controlled contacting. ofgases with liquids. at. a predetermined temperature which may be as high as750." F. ormore and at an extremely high pressure which. may .be inthe range of 2,000 to 15,000 pounds per square inch. The apparatus consists essentially .of two readily separable parts, namely; v(A) aheater and support; and. (B) areactor withitsassociated contacting means. The heaterand support consists of asection of 6-inch (schedule 40) steel pipe-.10, about 18. inches long, weldedto a .fianged support H, which maybe bolted .to a work bench orthe like. A 3% inch I. .D. stainless steel tube 12, inch thick and about 4%. inches long is welded .toflangel3, which may be screwed .to the top of pipe 0. To the rounded bottom portion of. pipe 12 .is welded a. 31-inch O. D. stainless steel .tube Hi, about inch thick and fiinches long, lugs J5 .beingprovided at the junctureof these two pipes for supporting the reactor assembly. A

threaded through said flange.

conical base i6 is welded to the base of tube 4 at its upper end and at its base to a inch stainless steel pipe 11, 1 inch long, the latter being provided with a Y-pipe connection 18 for drain hose l9, and also being provided with a ring and packing nut assembly 20 for receiving the thermowell casing 2! of the reactor. A 24 gauge 18-8 stainless steel sheath 22 extends downwardly from pipe l2 and together with the annular base 23 of similar metal forms a chamber for heating coils 24, which in this case, consists of approximately 20 feet of No. 22 Nichrome wire insulated with one-quarter inch diameter fishspine beads. The ends of the wire are passed through porcelain tubes 25 through base 23 and through pipe H} for connection to a power source, this particular heater 24 being of about GOO-watt capacity.

The space between pipe I0 and the stainless steel sheath 22 is preferably filled with magnesia,

' vermiculite, or other suitable insulation material 2B, and the temperature of this space may be measured by a thermocouple or other suitable means introduced into thermowell 2'1.

that the reactor may be quickly quenched, a gas- In order eous cooling fluid may be introduced by communication 28 passing up through the annulus between the exterior of the reactor 3| and the inside wall of the heater tube i4. Liquid coolants,

such as cold water, may be introduced through specially fabricated Glass-Col heating mantel for lightweight flexibility in use.

The reactor or contractor 3! is formed chiefly by pressure vessel Walls 32 which may be of about inch thick with an inside diameter of about 1% inches and a height of about 6 inches. The notched upper and inner edge of the reactor is provided with a gasket 33 of copper or other suitable metal against which the reactor head 34 is secured by closure cap 35, the pressure exerted by the inner flange thereof being equalized by a thrust plate ring 38 and suitable bolts 31 The reactor head 34 may be provided with a suitable high pressure connecting ring fitting 38 carrying 2 or more ports, one of which, 39, is shown connected to a small separate conduit or bore 40 in the head. The other ports (not shown) connect directly to an axial conduit or bore 4|. Reaotants or any fluid may be introduced into the reactor through any of these ports, and one of them is preferably attached to a refrangible safety disk holder with disk (not shown) designed to burst at 50% over the reaction pressure. Bore 4| is provided for the stem 42 of mixer 43 and in the upper part of the reactor head 34, bore 4! leads into a larger diameter bore 44 to accommodate magnetic core 45 which is secured at its base to stem 42. A lower spring 46 cushions the lowermost movement of the core, stem and stirrer blade 43 and prevents actual impingement of the latter against the base of the reactor, and upper spring 47 similarly cushions the uppermost movement of magnetic core 45.

The top of the reactor head 34 is closed by a connector 48 which forces the coned gland 49 into a cone seat cut in the top end of the reactor head. A standard high pressure cone seat fitting 50 in the top of the connector and gland then connects the reactor to a pressure gauge (not shown). The reactor head 34, stem 42 and springs 45 and 41 must be made of non-magnetic material, preferably stainless steel of austemtic structure, although copper, brass, and the like, non-magnetic materials may be used as well.

While the reactor closure here described is of the compression type, our invention is in no way restricted to this type closure, and any suitable closure such as the self-sealing type may be preferred especially at the higher pressures of 5000 p. s. i. and up.

The thermowell casing '21 extends upwardly into the bottom of the reactor, said casing having a shoulder 5! which is held in place by a gland nut 52 which is threaded to engage threads on a projecting lower end of the reactor walls. In reactors of larger size, the thermowell casin may depend from the reactor head instead of extending through its base.

Surrounding the upper end of the reactor head 34 are two solenoids 53 and 54. The current to the solenoid 53 is controlled by relay 55 and the current to solenoid 54 is controlled by relay 56. The current is applied alternately to each relay by a timer 56 which permits individual control of the on time of each. (A convenient commercially available relay and timer combination is offered by G. C. Wilson and Company, Chatham, N. J., as Repeat Cycle Timer Model No. l, with standard cycle time.) Any dual control timer which permits separate control of each cycle in the range 0.05 to 5 seconds would be suitable. By having two separate solenoid and having each solenoid separately controlled by an electronic timer, the movement of the stirrer is positively actuated in both upward and downward directions and it may be controlled with great precision. Various sizes and shapes of stirrers may, of course, be employed depending upon the viscosity of the fluids to be mixed. The movement of the mixer may likewise be controlled by changing the length of stem 42 or by employing suitable stops so that it remains constantly within a liquid phase in the reactor when it is desired to contact 2 immiscible liquids and so that it may move above the liquid level when it is desired to obtain contact between a gas and a liquid.

For obtaining intimate contact between a gas and a liquid and, particularly for recycling a gas from the upper part of the reactor to the bottom I thereof, a modification of our apparatus may be employed as illustrated in Figure 2 and Figure 3 which shows an enlarged View or the essential parts. In this case, one or more conduits 57 are provided in the walls of a small cylinder 58 which may be removably attached by screw thread to the reactor head 34 or may be integrally machined into the base of the reactor head 34, and tubes 59 extend these conduits to the base of the reactor. In this case, a larger opening is provided in the reactor head or attached cylinder '58 to serve as a gas receiver and a piston 6| is secured to stem 42, the piston being provided with one or more valves illustrated by opening 52,

plate ring 63, and plate retaining ring 54. With this apparatus when stem 42 is moved sharply in a downward direction the plate ring is disaes'aoar ing ring. 64) so tha'trthe space -above the. piston El is filledwith'gasz 1 During upward movement of stem 4Zthe entrapped gas'is forced through conduits "5! and 5S intothe base ofthe reactor. Mixer43 may optionally be attached to the piston El. by extension of'rod- 52 to stir liquid phase during. gasrecycling operation, mixer blades-43 being suitably apertured or spaced to avoid contact with tubes 59.

A further modification. of our apparatus for recycling gas from the upper part of the reactor to, and intimate dispersion otgas in, the liquid phase may be employed as: illustrated in Figure i. In this case, the stirrup type mixer in Figure l is modified by placing an inverted cup 65 of Suit". ablemesh screen over the connecting stirrup of mixer 43' and adjusting thestrolre of the mixer rod 42" so that the mixer 65 is lifted. above the liquidsurface into the gas phase where it fills with the gas. The meshes oi the screen are closed by liquid film due to surface tension effects, thus capturing a given volume of gas in theinverted cup. On the down stroke, the sudden submergence of mixer 55 causes the gas to bubble out through the meshes and escape to the surface ina fine spray with attendant beneficial effects of. intimate. contact of gas and liquid phases. Other shapes and forms of mixers, suitably perforated or meshed, maybe used, the above being cited merelyjas an example of the principle involved.

It will thus be seen that We have accomplished the objects of.,.our, invention. Furthermore; we have provided an apparatus with an improved safety feature by surrounding the reactor with the heating and-insulating chamber, which would absorb at least a substantial part of the shock should the contactor burst on account of failure of the safety disk to function. The stainless steel liner tube of the support permits water cooling of the reactor in case of emergency or if a reactor requires. quenching, the design also permits rapid air cooling of the reactor. A mostimport-v ant feature, however, is precision with which mixing can be accomplished by'positively and closely controlledmovement of the-magnetic core in both upward and downward direction by the electroni cally controlled pair of solenoids. Obviously. many variations in structure may be made. The solenoids may be slideably mounted on the narrowed, non-magnetic portion of the reactor head and held in any desired position by set screws. The reciprocating motion of the core may be translated by any known mechanism to provide rotary stirring. In sufficiently large reactors, the thermowell casing may suspend from the reactor head instead of being inserted at the base. These and other modifications will be apparent to those skilled in the art from the above description.

We claim:

1. Apparatus for contacting separate phases at controlled temperature and high pressure, which apparatus comprises a pressure vessel having an open top and closed base, a thermowell casing extending into the lower part of said vessel and removably secured therein, an elongated closure element for said pressure vessel of non-magnetic material provided with a bore communicating with said vessel and in substantial alignment therewith, a mixer element in said vessel, a movable magnetic core in said bore, a non-magnetic stem connecting said core to said mixer; a lower solenoid coaxial with said core in its lower position, an upper solenoid coaxial with said core in its upper position, said solenoids being in opposed tandem::arrangement-.and 'adaptedalternately. to lift and to depressth'e core, a timenfor'separately' controlling the energizing ofeach solenoid, and; means for securing said closure-element on said vessel.-

2. The apparatus of claim 1 in which the mixer-- vessel.-*

'3. "The apparatus of: claim 1 wherein the mixer consists essentially of a reciprocable element comprised of an inverted foraminous metal cup.

4.-The apparatus'of claim-1 wherein the mixer 1 element comprises a valved piston and a conduit I communicating from a space above "saidpiston to the bottom of-the vessel;

5.The apparatus of claim 1 wherein the pressure vessel is provided with an opening at its base: and a gland nut for mounting :the' thermowell' casing through said base.

S.-The apparatus of claim 1 wherein the elongated closure element is provided with a secondlongitudinal bore which" serves. as a conduit leading from-the exterior ofsaid. closure element into said vessel, a high pressure'connecting ring fit-I ting surrounding the elongated closure element adjacent the-outlet end of said second bore, and at-least one port in said ring fitting which communicates with the said outlet end of said second bore. r

'7. Contacting apparatus which 1 comprisesa pressure vessel with an open'top, an axially e1ongated closure element for-closing the" top of said vessel, said closure elementbeing providedwith 8. Apparatus for contacting separate'phases atcontrolled temperature and high pressure, which apparatus comprises a pressure vessel, a thermowell casing extending into the base of said vessel with an open top and aclosed base, a threaded opening through said base, and removably secured through said threaded opening, an elongated closure element for closing the top of said pressure vessel, said closure element having an elongated upper portion of non-magetic material, a bore in said elongated upper portion communicating with said vessel and in substantial alignment therewith, a mixer element in. said vessel, a movable magnetic core in said bore, a non-magnetic stem connecting said core to said mixer element, a lower solenoid substantially surrounding said core in its lower position, an upper solenoid substan tially surrounding said core in its upper position, a timer for separately controlling the energizing of each solenoid, a closure cap for securing said head on said vessel, and a heater support for said pressure vessel, said heater support comprising an annular insulated jacket, an upper inner wall of slightly larger inside diameter than the outside diameter of the securing means, a cap inner wall of slightly larger inside diameter than the outside diameter of the said pressure vessel, supports at the top of the lower walls for engagement with the lower part of the securing means, an electrical heating element surrounding the lower inner walls, a connection for introducing a fluid into the space between the lower walls, a connection for withdrawing fluid from said space, and a packing unit assembly for sealing the space between the lower walls and the thermowell casing.

9. An apparatus for effecting contact of separate phases in a closed high pressure vessel which apparatus comprises an open top pressure vessel, a non-magnetic elongated closure element for said pressure vessel provided with a bore in communication with said vessel and in substantial axial alignment therewith, a mixer element in said vessel, a movable magnetic core within said non-magnetic bore, a stem connecting said core and said mixer element, a pair of separately operable opposed solenoids coaxial with the elongated closure element of the pressure vessel in the region of said core, a relay means for controlling the energizing of said solenoids, and a heater-support for said pressure vessel including means for fixing a removable electrical heating element about the outer wall of said vessel.

10. Contacting apparatus which comprises a pressure vessel having side and bottom walls but open at its top, a closure element for the top of said pressure vessel, said closure element having an elongated upper portion, said elongated upper portion of said closure being of non-magnetic material and being provided with a bore which extends downwardly through said closure element and communicates with said vessel in substantial alignment therewith, mixing means in said vessel, a movable magnetic core in said bore, connecting means between said core and said mixing means whereby the latter is actuated by the former, and solenoid means for positively reciprocating said core within said bore, said solenoid means including a pair of solenoids arranged in opposed tandem relation co-axially about said bore.

11. The apparatus which comprises a pressure vessel having side and bottom walls but open at its top, a closure element for the top of said pressure vesel, said closure element having an elongated upper portion, said elongated upper portion of said closure being of non-magnetic material and being provided with a bore which extends downwardly through said closure element and communicates with said vessel in substantial alignment therewith, a reciprocable member in said vessel, a foraminous metal cup carried by said reciprocable member, a movable magnetic core in said bore, connecting means between said core and said reciprocable member whereby the latter is actuated by the former, and solenoid means for positively reciprocating said core with in said bore, said solenoid means including a pair of solenoids arranged in opposed tandem relation co-axially about said bore.

12. The apparatus which comprises a pressure vessel having side and bottom walls but open at its top, a closure element for the top of said pressure vessel, said closure element having an elongated upper portion, said elongated upper portion of said closure being of non-magnetic material and being provided with a bore which extends downwardly through said closure element and communicates with said vessel in substantial alignment therewith, a valved piston means in said vessel, conduit means communicating from a point above said piston to a point adjacent the bottom of the said vessel, a movable magnetic core in said bore, connecting means between said core and said piston means whereby the latter is actuated by the former, and solenoid means for positively reciprocating said core Within said bore, said solenoid means including a pair of solenoids arranged in opposed tandem relation coaxially about said bore.

WARD E. KUENI'ZEL. EDMUND FIELD.

REFERENCES GITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 417,611 Vogel Dec. 17, 1888 1,123,092 Calvert Dec. 29, 1914 1,472,281 Page Oct. 30, 1923 2,165,253 Graves July 11, 1939 2,223,348 Boedeker Dec. 3, 1940 

8. APPARATUS FOR CONTACTING SEPARATE PHASES AT CONTROLLED TEMPERATURE AND HIGH PRESSURE, WHICH APPARATUS COMPRISES A PRESSURE VESSEL, A THERMOWELL CASING EXTENDING INTO THE BASE OF SAID VESSEL WITH AN OPEN TOP AND A CLOSED BASE, A THREADED OPENING THROUGH SAID BASE, AND REMOVABLY SECURED THROUGH SAID THREADED OPENING, AN ELONGATED CLOSURE ELEMENT FOR CLOSING THE TOP OF SAID PRESSURE VESSEL, SAID CLOSURE ELEMENT HAVING AN ELONGATED UPPER PORTION OF NON-MAGETIC MATERIAL, A BORE IN SAID ELONGATED UPPER PORTION COMMUNICATING WITH SAID VESSEL AND IN SUBSTANTIAL ALIGNMENT THEREWITH, A MIXER ELEMENT IN SAID VESSEL, A MOVABLE MAGNETIC CORE IN SAID BORE, A NON-MAGNETIC STEM CONNECTING SAID CORE TO SAID MIXER ELEMENT, A LOWER SOLENOID SUBSTANTIALLY SURROUNDING SAID CORE IN ITS LOWER POSITION, AN UPPER SOLENOID SUBSTANTIALLY SURROUNDING SAID CORE IN ITS UPPER POSITION, A TIME FOR SEPARATELY CONTROLLING THE ENERGIZING OF EACH SOLENOID, A CLOSURE CAP FOR SECURING SAID HEAD ON SAID VESSEL, AND A HEATER SUPPORT FOR SAID PRESSURE VESSEL, SAID HEATER SUPPORT COMPRISING AN ANNULAR INSULATED JACKED, AN UPPER INNER WALL OF SLIGHTLY LARGER INSIDE DIAMETER THAN THE OUTSIDE DIAMETER OF THE SECURING MEANS, A CAP INNER WALL OF SLIGHTLY LARGER INSIDE DIAMETER THAN THE OUTSIDE DIAMETER OF THE SAID PRESSURE VESSEL, SUPPORTS AT THE TOP OF THE LOWER WALLS OF ENGAGEMENT WITH THE LOWER PART OF THE SECURING MEANS, AN ELECTRICAL HEATING ELEMENT SURROUNDING THE LOWER INNER WALLS, A CONNECTION FOR INTRODUCING A FLUID INTO THE SPACE BETWEEN THE LOWER WALS, A CONNECTION FOR WITHDRAWING FLUID FROM SAID SPACE, AND A PACKING UNIT ASSEMBLY FOR SEALING THE SPACE BETWEEN THE LOWER WALLS AND THE THERMOWELL CASING. 